Correlative Atom Probe Tomography and Transmission Electron Microscopy Analysis of Grain Boundaries in Thermally Grown Alumina Scale

Abstract

We employed correlative atom probe tomography (APT) and transmission electron microscopy (TEM) to analyze the alumina scale thermally grown on the oxide dispersion-strengthened alloy MA956. Segregation of Ti and Y and associated variation in metal/oxygen stoichiometry at the grain boundaries and triple junctions of alumina were quantified and discussed with respect to the oxidation behavior of the alloy, in particular, to the formation of cation vacancies. Correlative TEM analysis was helpful to avoid building pragmatically well-looking but substantially incorrect APT reconstructions, which can result in erroneous quantification of segregating species, and highlights the need to consider ionic volumes and detection efficiency in the reconstruction routine. We also demonstrate a cost-efficient, robust, and easy-handling setup for correlative analysis based solely on commercially available components, which can be used with all conventional TEM tools without the need to modify the specimen holder assembly.

Influence of codoping with Hf and La on grain‐boundary transport in alumina

“…This is not wholly unexpected given that APT is a more sensitive technique, and in HAADF‐STEM, the Z contrast is averaged down the length of each atomic column. Segregation of RE dopants have also been reported in other APT studies, but to date, the majority of these have been carried out on thermally grown oxide scales 53,54 . In this study, one key advantage of the APT was the ability to differentiate between the Hf and La ions in the GB region.…”

“…Segregation of RE dopants have also been reported in other APT studies, but to date, the majority of these have been carried out on thermally grown oxide scales. 53,54 In this study, one key advantage of the APT was the ability to differentiate between the Hf and La ions in the GB region. Based on ionic size one might expect La to segregate preferentially, but this does not appear to be the case.…”

Наноиндентирование И Механические Свойства Материалов В Субмикро- И Наношкале. Недавние Результаты И Достижения (О Б З О Р)

“…История исследования механических свойств твердых тел на микрообразцах восходит к 50-м годам прошлого века, когда впервые были выращены и испытаны искусственные нитевидные кристаллы [83], часто называемые усами или вискерами (от англ. whiskers), и опубликованы первые обзоры на эту тему [84][85][86] [112][113][114], повысившей пространственное разрешение до близкого к атомарному. Параллельно для in situ деформирования субмикрообразцов и нановолокон развивалась техника наномеханических испытаний.…”

“…In situ нано-/микро-механическим исследованиям деформационного поведения кристаллических, аморфных и нанокомпозитных материалов посвящен ряд обзоров, опубликованных в последнее десятилетие [114,[117][118][119]. Особенно отметим обширный многоплановый обзор [23] и энциклопедию современных подходов, методов и результатов исследования физико-механических свойств твердых тел и материалов самых различных классов в мультимасштабной размерной шкале от нано-до макро- [19].…”

Bulk and Short‐Circuit Anion Diffusion in Epitaxial Fe2O3 Films Quantified Using Buried Isotopic Tracer Layers

“…To overcome this limitation, information‐rich 3D composition maps of the elemental and isotopic distribution in solids can be obtained by atom probe tomography (APT) [ 51 ] with excellent areal and depth spatial resolution of <1 nm. These isotopically resolved compositional maps [ 13,52–54 ] make APT a promising technique to track the diffusion of both compositional [ 18,55,56 ] and isotopic [ 57–59 ] tracers at the nanoscale. For instance, Taylor et al.…”